CN101319124A - Environment friendly high-density aqueous woodenware emulsion paint and preparation method thereof - Google Patents
Environment friendly high-density aqueous woodenware emulsion paint and preparation method thereof Download PDFInfo
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- CN101319124A CN101319124A CNA2008101381132A CN200810138113A CN101319124A CN 101319124 A CN101319124 A CN 101319124A CN A2008101381132 A CNA2008101381132 A CN A2008101381132A CN 200810138113 A CN200810138113 A CN 200810138113A CN 101319124 A CN101319124 A CN 101319124A
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- 239000000839 emulsion Substances 0.000 title claims abstract description 102
- 238000002360 preparation method Methods 0.000 title claims abstract description 40
- 239000003973 paint Substances 0.000 title claims description 32
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 35
- 239000000178 monomer Substances 0.000 claims abstract description 34
- 239000011248 coating agent Substances 0.000 claims abstract description 32
- 238000000576 coating method Methods 0.000 claims abstract description 32
- 239000002904 solvent Substances 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000008367 deionised water Substances 0.000 claims abstract description 24
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 24
- 239000003999 initiator Substances 0.000 claims abstract description 24
- 239000000203 mixture Substances 0.000 claims abstract description 24
- 238000003756 stirring Methods 0.000 claims abstract description 20
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 16
- 238000009835 boiling Methods 0.000 claims abstract description 12
- 239000000080 wetting agent Substances 0.000 claims abstract description 12
- 239000000872 buffer Substances 0.000 claims abstract description 11
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 9
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 239000002562 thickening agent Substances 0.000 claims abstract description 4
- 239000002023 wood Substances 0.000 claims description 18
- 238000007599 discharging Methods 0.000 claims description 14
- 239000013530 defoamer Substances 0.000 claims description 11
- 230000008719 thickening Effects 0.000 claims description 11
- 239000003153 chemical reaction reagent Substances 0.000 claims description 10
- LVHBHZANLOWSRM-UHFFFAOYSA-N itaconic acid Chemical compound OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 9
- -1 alkyl ether ammonium sulfate Chemical class 0.000 claims description 8
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 claims description 7
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 7
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 7
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 6
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 6
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 6
- 239000003125 aqueous solvent Substances 0.000 claims description 6
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 6
- 238000010790 dilution Methods 0.000 claims description 6
- 239000012895 dilution Substances 0.000 claims description 6
- 230000003472 neutralizing effect Effects 0.000 claims description 6
- OAYXUHPQHDHDDZ-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethanol Chemical compound CCCCOCCOCCO OAYXUHPQHDHDDZ-UHFFFAOYSA-N 0.000 claims description 5
- CCJAYIGMMRQRAO-UHFFFAOYSA-N 2-[4-[(2-hydroxyphenyl)methylideneamino]butyliminomethyl]phenol Chemical compound OC1=CC=CC=C1C=NCCCCN=CC1=CC=CC=C1O CCJAYIGMMRQRAO-UHFFFAOYSA-N 0.000 claims description 5
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 claims description 5
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 5
- IBVAQQYNSHJXBV-UHFFFAOYSA-N adipic acid dihydrazide Chemical compound NNC(=O)CCCCC(=O)NN IBVAQQYNSHJXBV-UHFFFAOYSA-N 0.000 claims description 5
- 238000009413 insulation Methods 0.000 claims description 5
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 claims description 4
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 4
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 4
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 4
- BDERNNFJNOPAEC-UHFFFAOYSA-N n-propyl alcohol Natural products CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 4
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 4
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 4
- 239000007858 starting material Substances 0.000 claims description 4
- CUVLMZNMSPJDON-UHFFFAOYSA-N 1-(1-butoxypropan-2-yloxy)propan-2-ol Chemical compound CCCCOCC(C)OCC(C)O CUVLMZNMSPJDON-UHFFFAOYSA-N 0.000 claims description 3
- RWNUSVWFHDHRCJ-UHFFFAOYSA-N 1-butoxypropan-2-ol Chemical compound CCCCOCC(C)O RWNUSVWFHDHRCJ-UHFFFAOYSA-N 0.000 claims description 3
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 3
- 239000012874 anionic emulsifier Substances 0.000 claims description 3
- FQPSGWSUVKBHSU-UHFFFAOYSA-N methacrylamide Chemical compound CC(=C)C(N)=O FQPSGWSUVKBHSU-UHFFFAOYSA-N 0.000 claims description 3
- 229920002635 polyurethane Polymers 0.000 claims description 3
- 239000004814 polyurethane Substances 0.000 claims description 3
- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 claims description 3
- BWYYYTVSBPRQCN-UHFFFAOYSA-M sodium;ethenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C=C BWYYYTVSBPRQCN-UHFFFAOYSA-M 0.000 claims description 3
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 2
- 238000006116 polymerization reaction Methods 0.000 claims description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 2
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 2
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract 1
- 239000002518 antifoaming agent Substances 0.000 abstract 1
- 239000003431 cross linking reagent Substances 0.000 abstract 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 230000002159 abnormal effect Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 238000004132 cross linking Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 238000012827 research and development Methods 0.000 description 3
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 2
- 239000012296 anti-solvent Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- XMRUJYGYYCLRGJ-UHFFFAOYSA-N azanium;2-[2-[2-[2-(4-nonylphenoxy)ethoxy]ethoxy]ethoxy]ethyl sulfate Chemical compound [NH4+].CCCCCCCCCC1=CC=C(OCCOCCOCCOCCOS([O-])(=O)=O)C=C1 XMRUJYGYYCLRGJ-UHFFFAOYSA-N 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000004581 coalescence Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- WLEFRRNVWGUEIP-UHFFFAOYSA-N n-[bis(aziridin-1-yl)phosphoryl]-2-iodobenzamide Chemical compound IC1=CC=CC=C1C(=O)NP(=O)(N1CC1)N1CC1 WLEFRRNVWGUEIP-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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Abstract
The invention provides an environment-friendly high-density aqueous woodenware emulsion coating material and a preparation method thereof, belonging to the woodenware coating material technical field. The preparation method comprises the following steps that: firstly, an ordinary emulsifier, a buffer and solvent water are fed into a kettle and are heated to a temperature of between 80 and 82 DEG C; an ordinary emulsifier, a polymerisable emulsifier, nuclear monomer and deionized water are placed in another kettle to prepare an emulsion; an initiator solution is added in the kettle and is stirred evenly, and then a preemulsion is added in drops to prepare a seed emulsion; then, shell monomer and an initiator are dripped into the kettle together, and the temperature of the mixture is maintained at 84 to 86 DEG C for 1 hour; then, the mixture is cooled down and ammonia water is added; when the solution is cooled down to 45 DEG C, a crosslinking agent is added, and an aqueous woodenware emulsion is obtained after cooling, filtration and discharge and is fed into a stirring kettle; under the condition of stirring, a solvent, i.e. deionized water, a high boiling point solvent, a wetting agent and a antifoam agent are added in turn and are stirred and then a thickening agent is added to carry out defoaming slowly; and the aqueous woodenware emulsion coating material obtained after filtration and discharge has the characteristics of high hardness, excellent water resistance and solvent resistance and low VOC emission.
Description
Technical field
The present invention relates to the woodwork coating technical field, specifically a kind of environment friendly high-density aqueous woodenware emulsion paint and preparation method thereof.
Background technology
Further perfect along with environmental regulation is purpose to alleviate earth load, and the new coating of low VOC or zero VOC discharging becomes the focus of research and development, and the research and development of water-borne wood coating are more noticeable.
At present, European civilian coating has reached higher Water-borne modification level.Woodwork coating accounted for 8% of whole Europe coating sales volume in 1996, and surplus in the of about 40 ten thousand tons, wherein water-borne wood coating accounts for 6% of woodwork coating total amount.1999, European civilian coating ultimate production was 3,000,000 tons, and wherein water-miscible paint reaches 2,500,000 tons, accounts for 72%; The Water-borne modification of Northern European countries's Floor paint has reached 80%.
Recent years; China is very active about the research and development of water-borne wood coating technology; state of the art also improves very fast; especially the green of the 2008 Beijing Olympic Games, environmental protection concept; and the construction of a large amount of the Olympic stadiums all proposes very high requirement to environmental protection, for the large-scale application of environment-friendly type aqueous coating provides good chance.
It is reported that Chinese woodwork coating has the market of few hundred thousand tonnes of every year, if water-borne wood coating can replace the solvent-borne type woodwork coating, its environmental-protection function and economic results in society are very significant.
Current, ACRYLIC EMULSION is because the shortcoming of " hot sticky cold crisp ", and contains a large amount of emulsifying agents, it is water-fast, anti-solvent is not fine, owing in order to reach high rigidity, often need to improve second-order transition temperature, thereby increase the usage quantity of film coalescence aid, and do not reach the purpose of low VOC.
Summary of the invention
Technical assignment of the present invention is to solve the deficiencies in the prior art, a kind of environment friendly high-density aqueous woodenware emulsion paint and preparation method thereof is provided, and the synthetic ACRYLIC EMULSION with " nuclear-shell " type structure and high rigidity of a kind of specifically employing Polymerizable Emulsifier prepares the method for water-borne wood coating.
Technical scheme of the present invention realizes in the following manner, a kind of environment friendly high-density aqueous woodenware emulsion paint, and the starting material of this woodenware emulsion paint are as follows according to weight proportion:
(1) aqueous wooden ware emulsion:
Conventional emulsifier 0.1-1 monomer 20-80
Polymerizable Emulsifier 0.1-1 solvent 40-80
Initiator 0.01-0.6 neutralizing agent 0.2-1.5
Buffer reagent 0.01-0.1 linking agent 0.2-1.5;
(2) water-borne wood coating:
Aqueous wooden ware emulsion 60-100 wetting agent 0.1-1
Solvent 2-20 defoamer 0.1-2
High boiling solvent 2-20 thickening material 0.1-1.
The starting material of described woodenware emulsion paint are as follows according to the more preferably scheme of weight proportion:
(1) aqueous wooden ware emulsion:
Conventional emulsifier 0.3-0.5 monomer 37.8-54.6
Polymerizable Emulsifier 0.3-0.5 solvent 55-60
Initiator 0.1-0.3 neutralizing agent 0.5-0.8
Buffer reagent 0.03-0.05 linking agent 0.4-0.7;
(2) water-borne wood coating:
Aqueous wooden ware emulsion 70-90 wetting agent 0.1-1
Solvent 5-15 defoamer 0.1-2
High boiling solvent 5-15 thickening material 0.1-1.
Described conventional emulsifier comprises anionic emulsifier, comprises one or more mixtures in Sodium dodecylbenzene sulfonate, sodium laurylsulfonate, the ethoxylated alkyl ether ammonium sulfate;
Described Polymerizable Emulsifier comprises one or more mixtures in allyloxy Nonylphenoxy propyl alcohol polyoxyethylene ether ammonium sulfate, sodium vinyl sulfonate, the allyl group alkylphenol polyoxyethylene vitriol;
Described monomer comprises one or more mixtures in vinyl cyanide, methacrylic acid, methylene-succinic acid, acrylamide, methyl methacrylate, butyl acrylate, diacetone-acryloamide(DAA), Methacrylamide, the N hydroxymethyl acrylamide; Employing has the monomer of special functionality, to improve the degree of crosslinking of emulsion, to improve the emulsion solvent resistance;
Described aqueous solvent comprises deionized water; Described initiator comprises Sodium Persulfate; Described buffer reagent comprises sodium bicarbonate; Described neutralizing agent comprises ammoniacal liquor; Described linking agent comprises adipic dihydrazide.
Described monomer is divided into nuclear monomer and shell monomer according to the polymerization characteristics, and wherein: nuclear monomer comprises one or more mixtures in methyl methacrylate, butyl acrylate, vinyl cyanide, methylene-succinic acid, the N hydroxymethyl acrylamide; Shell monomer comprises one or more mixtures in methyl methacrylate, butyl acrylate, vinyl cyanide, methacrylic acid, the diacetone-acryloamide(DAA).
Introducing Polymerizable Emulsifier can be allyloxy Nonylphenoxy propyl alcohol polyoxyethylene ether ammonium sulfate, sodium vinyl sulfonate, allyl group alkylphenol polyoxyethylene vitriol etc., reduces the consumption of conventional emulsifier;
Conventional emulsifier is an anionic emulsifier, can be Sodium dodecylbenzene sulfonate, sodium laurylsulfonate, A-103, CO-436 etc.;
Adopt " nuclear-shell " polymeric technology,, reduce the film forming auxiliary dosage to be lowered into film temperature;
By the monomer that adopts vinyl cyanide, methacrylic acid, methylene-succinic acid, acrylamide, Methacrylamide, N hydroxymethyl acrylamide etc. to have special functionality, to improve the degree of crosslinking of emulsion, to improve the emulsion solvent resistance;
Adopt the ambient cure of diacetone-acryloamide(DAA) and adipic dihydrazide crosslinked, further improve the film forming degree of crosslinking.
A kind of environment friendly high-density aqueous woodenware emulsion paint of the present invention and preparation method thereof comprises the preparation of aqueous wooden ware emulsion and utilizes the aqueous wooden ware emulsion of preparation to prepare aqueous woodenware emulsion paint that its method is:
(1) preparation method of aqueous wooden ware emulsion:
Earlier conventional emulsifier, buffer reagent, aqueous solvent are dropped at the bottom of the still heat temperature raising to 70 ℃-90 ℃; In another jar, add conventional emulsifier, Polymerizable Emulsifier, nuclear monomer, deionized water and prepare pre-emulsion; The initiator solution that adds 1/5-1/2 is to still, after stirring, the pre-emulsion that adds 1/5-3/5 prepares seed emulsion, dripping the residue pre-emulsion time behind the 5min-20min is controlled at 1.5h-2.5h and drips off, the time that then shell monomer and initiator splashed into jointly to the still is controlled at 0.5h-1.5h and drips off, the dropping time is controlled at 2h-4h altogether, temperature is controlled at 80 ℃-90 ℃, insulation 1h is cooled to 55-70 ℃ then, adds in the ammoniacal liquor and arrives 7.0-8.0 with pH value, be cooled to 40 ℃-50 ℃ again, add linking agent, cooling, filtration discharging get the aqueous wooden ware emulsion;
(2) utilize the aqueous wooden ware emulsion to prepare the method for water-borne wood coating:
The aqueous wooden ware emulsion of preparation is added in the stirring tank, under the condition of 500rpm-700rpm, add solvent deionized water, high boiling solvent, wetting agent, defoamer successively, under 1000rpm, stir 25min-35min, then thickening material is adjusted viscosity with deionized water dilution back, froth breaking 30min filters discharging and makes aqueous woodenware emulsion paint at a slow speed.
The preferred version of a kind of environment friendly high-density aqueous woodenware emulsion paint of the present invention and preparation method thereof is:
(1) preparation method of aqueous wooden ware emulsion:
Earlier conventional emulsifier, buffer reagent, aqueous solvent are dropped at the bottom of the still heat temperature raising to 80 ℃-82 ℃; In another jar, add conventional emulsifier, Polymerizable Emulsifier, nuclear monomer, deionized water and prepare pre-emulsion; The initiator solution that adds 1/5-1/2 is to still, after stirring, add the 1/5-3/5 pre-emulsion and prepare seed emulsion, dripping the residue pre-emulsion time behind the 15min is controlled at 2h and drips off, the time that then shell monomer and remaining initiator splashed into jointly to the still is controlled at 1h and drips off, the dropping time is controlled at 3h altogether, temperature is controlled at 84 ℃-86 ℃, insulation 1h is cooled to 60 ℃-65 ℃ then, adds in the ammoniacal liquor and arrives 7.0-8.0 with pH value, be cooled to 45 ℃ again, add linking agent, cooling, filtration discharging get the aqueous wooden ware emulsion;
(2) utilize the aqueous wooden ware emulsion to prepare the method for water-borne wood coating:
The aqueous wooden ware emulsion of preparation is added in the stirring tank, under the condition of 600rpm, add solvent deionized water, high boiling solvent, wetting agent, defoamer successively, under 1000rpm, stir 30min, then thickening material is adjusted viscosity with deionized water dilution back, froth breaking 30min filters discharging and makes aqueous woodenware emulsion paint at a slow speed.
Described wetting agent comprises one or more mixtures among Hydropalat 140, Hydropalat 875, the BYK-346;
Described high boiling solvent comprises one or more mixtures in butyl glycol ether, Diethylene Glycol butyl ether, propylene glycol butyl ether, the dipropylene glycol butyl ether;
Described defoamer comprises one or more mixtures among Dehydran 1293, Foamstar A32, Foamstar A34, BYK-019, BYK-024, the BYK-025;
Described thickening material adopts the non-ionic polyurethane associative thickener, comprises one or more mixtures among DSX 1550, DSX 3256, the SN-612.
Described wetting agent can be Hydropalat 140, the Hydropalat 875 of Kening Co.,Ltd, one or more mixtures among the BYK-346 of BYK company etc.;
Described high boiling solvent can be one or more mixtures in butyl glycol ether, Diethylene Glycol butyl ether, propylene glycol butyl ether, the dipropylene glycol butyl ether etc.;
Described defoamer can be Dehydran 1293, Foamstar A32, the FoamstarA34 of Kening Co.,Ltd, one or more mixtures in the serial defoamers such as the BYK-019 of BYK company, BYK-024, BYK-025;
Described thickening material can be DSX 1550, the DSX 3256 of nonionic polyurethane associative thickener such as Kening Co.,Ltd, one or more mixtures among the SN-612 of NOPCO company etc.
The positively effect that a kind of environment friendly high-density aqueous woodenware emulsion paint of the present invention and preparation method thereof is compared with prior art produced is:
Use the prepared aqueous woodenware emulsion paint that goes out of the preparation method of this environment friendly high-density aqueous woodenware emulsion paint, water-fast, solvent resistance good, and have the characteristics of high rigidity.The use of Polymerizable Emulsifier in the preparation process, can reduce the usage quantity of conventional emulsifier in a large number, reduce conventional emulsifier to water-fast, the solvent-proof influence of film forming, adopt " nuclear-shell " polymeric technology simultaneously, reach and be lowered into film temperature, reducing the purpose of film forming auxiliary dosage, is the new coating of realizing preparing minimum VOC discharging.
Embodiment
Below a kind of environment friendly high-density aqueous woodenware emulsion paint of the present invention and preparation method thereof is done following detailed description the in detail.
Provide the most preferred embodiment of implementing a kind of environment friendly high-density aqueous woodenware emulsion paint of the present invention and preparation method thereof below:
Embodiment 1:
Aqueous wooden ware emulsion preparation synthesizing formula is as follows:
Preparation method: at the bottom of 4.8g Sodium dodecylbenzene sulfonate, sodium bicarbonate, 637g deionized water input still, be heated to 80 ℃-82 ℃, adding residue 2.4g Sodium dodecylbenzene sulfonate, allyloxy Nonylphenoxy propyl alcohol polyoxyethylene ether ammonium sulfate, nuclear monomer prepare pre-emulsion in another jar again.With the 80g deionized water initiator is dissolved, the preparation initiator solution, the initiator solution of adding 1/3 is to still, after stirring, add the 18g pre-emulsion and prepare seed emulsion, drip the about 2h of pre-emulsion behind the 15min, drip the about 1h of shell monomer then, the residue initiator solution follows monomer to drip off, and the dropping time is 3h altogether, temperature control is at 84 ℃-86 ℃, be incubated 1 hour, lower the temperature 60 ℃-65 ℃, arrive 7.0-8.0 with pH value in the ammoniacal liquor, be cooled to 45 ℃, add adipic dihydrazide.Cooling, filtration discharging, getting little yellow translucent liquid promptly is the aqueous wooden ware emulsion.
The median size of the aqueous wooden ware emulsion of preparing is 80nm, and viscosity is 300cps, and PH=7.5, solid content are 41.3%.
Use the aqueous wooden ware emulsion of preparation, preparation water-borne wood coating prescription is as follows:
Preparation method: the aqueous wooden ware emulsion of preparation is added in the stirring tank, at the material that adds the described sequence number 2-6 of table under the condition of 600rpm successively, that is: deionized water, butyl glycol ether, Diethylene Glycol butyl ether, Hydropalat 140, Dehydran 1293, under 1000rpm, stir 30min, then SN-612 is adjusted viscosity with deionized water dilution back, froth breaking 30min filters discharging and gets aqueous woodware paint at a slow speed.
The water-borne wood coating performance that makes: outward appearance is little yellow translucent liquid, and solid content is 33%, and viscosity (being coated with 4 glasss) is 30 seconds, surface drying time: 15min.The woodenware film forming properties: the pencil hardness of filming is H, water tolerance: 48 hours no abnormal, and alcohol resistance (50% ethanol): 1h is no abnormal, sticking power: 1 grade.
Embodiment 2:
Aqueous wooden ware emulsion preparation synthesizing formula is as follows:
Preparation method: at the bottom of 4.8g Sodium dodecylbenzene sulfonate, sodium bicarbonate, 637g deionized water input still, be heated to 80 ℃-82 ℃, adding residue 2.0g Sodium dodecylbenzene sulfonate, allyl group alkylphenol polyoxyethylene vitriol, nuclear monomer prepare pre-emulsion in another jar again.With the 80g deionized water initiator is dissolved, the preparation initiator solution, the initiator solution of adding 1/3 is to still, after stirring, add the 18g pre-emulsion and prepare seed emulsion, drip the about 2h of pre-emulsion behind the 15min, drip the about 1h of shell monomer then, the residue initiator solution follows monomer to drip off, and the dropping time is 3h altogether, temperature control is at 84 ℃-86 ℃, insulation 1h lowers the temperature 60 ℃-65 ℃, arrives 7.0-8.0 with pH value in the ammoniacal liquor, be cooled to 45 ℃, add adipic dihydrazide.Cooling, filtration discharging, getting little yellow translucent liquid promptly is the aqueous wooden ware emulsion.
The median size of the aqueous wooden ware emulsion of preparing is 85nm, and viscosity is 500cps, and PH=7.5, solid content are 41.3%.
Use the aqueous wooden ware emulsion of preparation, preparation water-borne wood coating prescription is as follows:
Preparation method: the aqueous wooden ware emulsion of preparing is added in the stirring tank, at the material that adds the described sequence number 2-6 of table under the condition of 600rpm successively, that is: deionized water, butyl glycol ether, Diethylene Glycol butyl ether, Hydropalat 875, BYK-025, under 1000rpm, stir 30min, rotating speed is transferred to 600rpm, then DSX-1550 is adjusted viscosity with deionized water dilution back, froth breaking 30min filters discharging and gets water-borne wood coating at a slow speed.
The water-borne wood coating performance that makes: outward appearance is little yellow translucent liquid, and solid content is 33%, and viscosity (being coated with 4 glasss) is 35 seconds, surface drying time: 15min.The woodenware film forming properties: the pencil hardness of filming is H, water tolerance: 48 hours no abnormal, and alcohol resistance (50% ethanol): 1h is no abnormal, sticking power: 1 grade.
Wherein the characterization method of each character among embodiment 1 and the embodiment 2 is:
(1) size and distribution: adopt Ma Erwen laser particle diameter instrument to measure;
(2) hardness, sticking power, anti-solvent: measure by the method that provides among the standard HG/T 3828-2006.
Claims (7)
1, a kind of environment friendly high-density aqueous woodenware emulsion paint is characterized in that the starting material of this woodenware emulsion paint are as follows according to weight proportion:
(1) aqueous wooden ware emulsion:
Conventional emulsifier 0.1-1 monomer 20-80
Polymerizable Emulsifier 0.1-1 solvent 40-80
Initiator 0.01-0.6 neutralizing agent 0.2-1.5
Buffer reagent 0.01-0.1 linking agent 0.2-1.5;
(2) water-borne wood coating:
Aqueous wooden ware emulsion 60-100 wetting agent 0.1-1
Solvent 2-20 defoamer 0.1-2
High boiling solvent 2-20 thickening material 0.1-1.
2, a kind of environment friendly high-density aqueous woodenware emulsion paint according to claim 1 is characterized in that the starting material of this woodenware emulsion paint are as follows according to weight proportion:
(1) aqueous wooden ware emulsion:
Conventional emulsifier 0.3-0.5 monomer 37.8-54.6
Polymerizable Emulsifier 0.3-0.5 solvent 55-60
Initiator 0.1-0.3 neutralizing agent 0.5-0.8
Buffer reagent 0.03-0.05 linking agent 0.4-0.7;
(2) water-borne wood coating:
Aqueous wooden ware emulsion 70-90 wetting agent 0.1-1
Solvent 5-15 defoamer 0.1-2
High boiling solvent 5-15 thickening material 0.1-1.
3, a kind of environment friendly high-density aqueous woodenware emulsion paint according to claim 1 and 2 is characterized in that:
Conventional emulsifier comprises anionic emulsifier, comprises one or more mixtures in Sodium dodecylbenzene sulfonate, sodium laurylsulfonate, the ethoxylated alkyl ether ammonium sulfate;
Polymerizable Emulsifier comprises one or more mixtures in allyloxy Nonylphenoxy propyl alcohol polyoxyethylene ether ammonium sulfate, sodium vinyl sulfonate, the allyl group alkylphenol polyoxyethylene vitriol;
Monomer comprises one or more mixtures in vinyl cyanide, methacrylic acid, methylene-succinic acid, acrylamide, methyl methacrylate, butyl acrylate, diacetone-acryloamide(DAA), Methacrylamide, the N hydroxymethyl acrylamide;
Aqueous solvent comprises deionized water; Initiator comprises Sodium Persulfate; Buffer reagent comprises sodium bicarbonate; Neutralizing agent comprises ammoniacal liquor; Linking agent comprises adipic dihydrazide.
4, according to claim 1,2 or 3 described a kind of environment friendly high-density aqueous woodenware emulsion paints, it is characterized in that:
Monomer is divided into nuclear monomer and shell monomer according to the polymerization characteristics, and wherein: nuclear monomer comprises one or more mixtures in methyl methacrylate, butyl acrylate, vinyl cyanide, methylene-succinic acid, the N hydroxymethyl acrylamide; Shell monomer comprises one or more mixtures in methyl methacrylate, butyl acrylate, vinyl cyanide, methacrylic acid, the diacetone-acryloamide(DAA).
5, a kind of method for preparing the described environment friendly high-density aqueous woodenware emulsion paint of claim 1 is characterized in that comprising the preparation of aqueous wooden ware emulsion and utilizes the aqueous wooden ware emulsion of preparation to prepare aqueous woodenware emulsion paint, and its method is:
(1) preparation method of aqueous wooden ware emulsion:
Earlier conventional emulsifier, buffer reagent, aqueous solvent are dropped at the bottom of the still heat temperature raising to 70 ℃-90 ℃; In another jar, add conventional emulsifier, Polymerizable Emulsifier, nuclear monomer, deionized water and prepare pre-emulsion; The initiator solution that adds 1/5-1/2 is to still, after stirring, the pre-emulsion that adds 1/5-3/5 prepares seed emulsion, dripping the residue pre-emulsion time behind the 5min-20min is controlled at 1.5h-2.5h and drips off, the time that then shell monomer and initiator splashed into jointly to the still is controlled at 0.5h-1.5h and drips off, the dropping time is controlled at 2h-4h altogether, temperature is controlled at 80 ℃-90 ℃, insulation 1h is cooled to 55-70 ℃ then, adds in the ammoniacal liquor and arrives 7.0-8.0 with pH value, be cooled to 40 ℃-50 ℃ again, add linking agent, cooling, filtration discharging get the aqueous wooden ware emulsion;
(2) utilize the aqueous wooden ware emulsion to prepare the method for water-borne wood coating:
The aqueous wooden ware emulsion of preparation is added in the stirring tank, under the condition of 500rpm-700rpm, add solvent deionized water, high boiling solvent, wetting agent, defoamer successively, under 1000rpm, stir 25min-35min, then thickening material is adjusted viscosity with deionized water dilution back, froth breaking 30min filters discharging and makes aqueous woodenware emulsion paint at a slow speed.
6, the preparation method of a kind of environment friendly high-density aqueous woodenware emulsion paint according to claim 5 is characterized in that:
(1) preparation method of aqueous wooden ware emulsion:
Earlier conventional emulsifier, buffer reagent, aqueous solvent are dropped at the bottom of the still heat temperature raising to 80 ℃-82 ℃; In another jar, add conventional emulsifier, Polymerizable Emulsifier, nuclear monomer, deionized water and prepare pre-emulsion; The initiator solution that adds 1/5-1/2 is to still, after stirring, add the 1/5-3/5 pre-emulsion and prepare seed emulsion, dripping the residue pre-emulsion time behind the 15min is controlled at 2h and drips off, the time that then shell monomer and remaining initiator splashed into jointly to the still is controlled at 1h and drips off, the dropping time is controlled at 3h altogether, temperature is controlled at 84 ℃-86 ℃, insulation 1h is cooled to 60 ℃-65 ℃ then, adds in the ammoniacal liquor and arrives 7.0-8.0 with pH value, be cooled to 45 ℃ again, add linking agent, cooling, filtration discharging get the aqueous wooden ware emulsion;
(2) utilize the aqueous wooden ware emulsion to prepare the method for water-borne wood coating:
The aqueous wooden ware emulsion of preparation is added in the stirring tank, under the condition of 600rpm, add solvent deionized water, high boiling solvent, wetting agent, defoamer successively, under 1000rpm, stir 30min, then thickening material is adjusted viscosity with deionized water dilution back, froth breaking 30min filters discharging and makes aqueous woodenware emulsion paint at a slow speed.
7, the preparation method of a kind of environment friendly high-density aqueous woodenware emulsion paint according to claim 5 is characterized in that:
Described wetting agent comprises one or more mixtures among Hydropalat 140, Hydropalat 875, the BYK-346;
Described high boiling solvent comprises one or more mixtures in butyl glycol ether, Diethylene Glycol butyl ether, propylene glycol butyl ether, the dipropylene glycol butyl ether;
Described defoamer comprises one or more mixtures among Dehydran 1293, Foamstar A32, Foamstar A34, BYK-019, BYK-024, the BYK-025;
Described thickening material adopts the non-ionic polyurethane associative thickener, comprises one or more mixtures among DSX 1550, DSX 3256, the SN-612.
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